Method of dissolving titanium tetrachloride in aqueous solvents



Patented Feb. 28, 1933 UNITED STATES PATENT OFFICE PAUL KUBELKA, OFPRAGUE, CZECHOSLOVAKIA, ASSIGNOR TO KREBS PIG-KENT &; COLOR CORPORATION,OF NEWARK, NEW JERSEY, A CORPORATION OF DELAWARE METHOD OF DISSOLVINGTITANIUM TETRACHLORIDE IN AQUEOUS SOLVENTS No Drawing. Application filedFebruary 12, 1932, Serial No. 592,656, and in Germany February 27, 1931.

The present invention relates to the production of solutions containingtitanium chloride and comprises introducing anhydrous titaniumtetrachloride into the body and below the surface of an aqueous solvent.

In the preparation of hydrochloric acid solutions containing titanium by.mixing titanium tetrachloride with water or with an aqueous solution,local overheating usually occurs due to the high heat of solution whichresults in an evaporation of titanium tetrachloride and consequent lossof this material.

The volatilization losses can be reduced by a vigorous agitation of thesolvent but cannot be entirely avoided in this manner.

I have found that the losses of evaporation can practically completelybe avoided if the titanium tetrachloride is introduced below the surfaceof the suitably agitated solvent. This may be accomplished by using oneor more submerged feed pipes for the titanium chloride. It wasunexpectedly found that no clogging up of these feed pipes by titaniumoxygen compounds or titanium oxychlorides takes place or that therelatively small pressure of a titanium chloride column of a fewdecimeters is sufiicient to remove such precipitates from the pipes. Iobtain in this manner of introducing the titanium tetrachloride into thesolvent, particularly when the solvent is simultaneously vigorouslyagitated, a much more uniform distribution of the heat as has beenachieved up to the present time by the usual introduction of thetitanium chloride on the surface of the solvent. The hydrochloric acidgas and steam which are evolved in this operation are practically freefrom titanium tetrachloride.

I further found it advisable, in this manner of introducing titaniumtetrachloride into a solvent, to pass through these submerged feed pipesa current of dry air or other inert gas together with the titaniumtetrachloride whereby not only the backing up of the tita= nium chloridein the pipes is prevented, but

this current of air further minimizes the I danger of clogging up thepipes by precipi tates.

As solvents for the tetrachloride, I can use, besides water,particularly hydrochloric acid and dilute solutions of titaniumtetrachloride.

I can also make the dissolution of the titanium tetrachloride in acontinuous manner by simultaneously introducing into a body of anaqueous solvent the titanium chloride and the solvent each of the twothrough one or more separate submerged feed pipes. The

dissolution vessel is also provided with an overflow so that the freshlyformed'titanium chloride solution is constantly removed. ;In

this case also I can add a little air to the stream of titaniumtetrachloride introduced. The rate of addition of the titaniumtetrachloride and that of the water, hydrochloric acid, titaniumchloride solution or other solvent,is regulated according to the desiredconcentration of the titanium chloride solution.

Evaporation losses of tetrachloride are in this case also, particularlywhen the solvent is vigorously agitated practically avoided.

I claim: 7

1. In a process for the preparation of a titanium chloride solution, thestep which comprises introducing titanium tetrachloride into an agitatedaqueous solvent below the surface of said solvent. I

2. In a process of preparing titanium chloride solutions, the step whichcomprises ride solution below the surface of said solu:

tion continuously withdrawing from the said body titanium chloridesolution and regulating the rate of introduction of said titaniumtetrachloride and said solvent so as to give the desired concentrationof titanium chloride in the solution.

In testimonywhereof, I' afiix my signature.

PAUL KUBELKA.

